对称双吡咯甲烷的合成与分子内氢键的研究

５－甲基吡咯－２－羧酸酯在磺酰氢，溴或四乙酸铅作用下，生成相应的在５－甲基上含取代基的产物，后者不经分离不便可自缩合得标题化合物，核磁共振氢谱研究和分子构象木匠，当３，３位的取代基为甲酸（酯）基或乙酸（酯）基时，可形成３，３位酯基与另一吡咯环上的氮氢之间的分子内氢键，而３，３位是其它取代基，如乙酰基，丙酸（酯）基，丁酸（酯）基时不能形成类似的分子内氢键。     

THE ELECTRON-BEAM IRRADIATION ON THE HIGH TEMPERATURE SUPERCONDUCTING THIN FILMS: A NUMERICAL SIMULATION OF THE LOW TEMPERATURE SCANNING ELECTRON MICROSCOPY

Low-temperature scanning electron microscopy (LTSEM) is a promising measuring technique for probing the spatial distribution of the superconducting properties of the high-temperature superconducting (HTS) thin films. A theoretical analysis of the electron-beam irradiation on the HTS thin films in the LTSEM has been carried out. An inhomogeneously distributed grain array model has been applied in the analysis, and some numerical sim-ulations have been carried out on the electron-beam induced voltage (EIV) signals in the LTSEM experiments. The comparisons of our numerical results with the LTSEM experi-mental data indicate that it is quite reasonable to use a two-dimensional Josephson junction array for stimulating the inhomogeneous HTS thin film sample. Our numerical results also show that the EIV signals are influenced by the electron-beam power used in the LTSEM, and a reduction of the electron-beam power is suggested in order to eliminate the errors in estimating the local values of critical temperature T_c and critical current I_c by the sample temperature and the bias current at which the first EIV signal occurs.     

非相干光源用于“核-环比”法测量表面粗糙度

本文将文献[1-5]的用激光测量表面粗糙度的“核-环比”法推广到采用其他非相干光源,给出测量原理的定量公式及测量装置的结构框图。     

一维螺旋状3，6-哒嗪二甲酸镉(Ⅱ)配位聚合物的合成与结构

Using the ligand pyridazine-3，6-dicarboxylate (H₂pzdc)， a coordination polymer [Cd₂(pzdc)₂(H₂O)₄] was synthesized and characterized by elemental analysis， thermal analysis， IR and single-crystal X-ray diffraction. The complex crystallizes in the tetragonal system with space group I4₁/a. The crystallographic data are: a=1.470 6(4) nm， c=1.489 8(6) nm， V=3.222 0(19) nm³， Z=16， μ=2.725 mm^-1， D_c=2.594 g·cm^-3， R₁=0.017 8， wR₂=0.044 6. In the complex， the cadmium(Ⅱ) ions with the eight-coordinated dodecahedral geometry are linked by the pzdc ligands to generate one-dimensional chains， which are associated into the three-dimensional architecture via O-H…O hydrogen bonding. CCDC: 658853.     

虾仁中氯霉素残留量的气相色谱测定

建立了用配有电子俘获检测器(ECD)的气相色谱仪来测定虾仁中的氯霉素含量的方法.试样用乙酸乙酯提取,正己烷去杂,硅胶柱纯化,BSTFA+TMCS(99:1)试剂硅烷化.以GC ECD方式测定,外标法定量.当添加水平为0.2×10-9～1.0×10-9μg/kg时,回收率为70%～110%;相对标准偏差为1.0%～5.0%;线性相关系数r大于0.998.     

引发甲基丙烯酸甲酯聚合的聚丙烯酰胺－氯化铜配合物膜催化剂表征

考察甲基丙烯酸甲酯在室温Ｎａ２ＳＯ３水溶液的聚合能力，发现在该溶液添加聚丙烯酰胺（ＰＡＡｍ）－氯化铜（ＣｕＣｌ２）配合物膜以组成ＰＡＡｍ－ＣｕＣｌ２膜／Ｎａ２ＳＯ３催化引发系是必不可少的，采用ＥＳＲ、ＩＲ、ＸＰＳ和电导率等手段研究该体系催化剂的表面结构，结果表明，膜的单位面积平均含铜量在一定范围内和配位体种类等对催化活性有显著影响，即催化性能与催化剂的表面结构紧密相关。     

STUDY ON LONG CHAIN BRANCHING IN POLYBUTADIENES BY GPC COUPLED WITH CAPILLARY VISCOMETER

The long chain branching of polybutadienes (PB) was measured with gel permeation chroma-tography coupled to an automatically recording capillary viscometer. In this method the experimentalrelation [η] (V) was translated into the calibration curve [η] (V_R) for the monodisperse species. The curve is combined with the universal calibration so that the molecular weight distributionand an additional parameter, e.g. the average branching factor of this samples may be obtained. Longchain branching molecular weight changes with polyemerization conditions.     

Li+粘贴CHnCl3-nO2和CFnCl3-nO2( n = 1~3 )自由基：Li+–CHnCl3-nO2和 Li+–CFnCl3-nO2的结构与性质的研究

The structures and stabilities of these still experimentally unknown CH_nCl_(3-n)O_(2-)Li~ and CF_nCl_(3-n)O_(2-)Li~ ionshave been theoretically investigated by ab initio molecular orbital theory and density functional theory(DFT)inconjunction with the 6-311G(d,p),6-311 G(d,p),6-311 G(2d,p)and 6-311 G(2df,2p)basis sets.The optimizedgeometries,chemical bonding and NBO analysis indicate that these complexes of CH_nCl_(3-n)O_(2-)Li~ and CF_nCl_(3-n)O_(2-)Li~ exist as ion-dipole molecules.The calculated affinity energies of these species exceed 41.9 kJ/mol,which arelarge enough to suggest the possibility that these title complexes could be detected as stable species in gas phase byLi~ ion attachment mass spectrometry.     

载气气氛对Co/MgMoO4催化剂CVD法高效合成碳纳米材料的影响

High yield and quality mutli-walled carbon nanotube (MWNT) bundles and carbon nanofibers were synthesized by catalytic decomposition of methane over Co/MgMoO₄ catalyst at 1 000 ℃. TEM studies showed that the products were mainly carbon nanofibers without carrier gas and were all MWNT bundles with hydrogen or nitrogen as carrier gas. Thermal gravimetric analyses (TGA) on the raw product indicated that the purity of MWNT was higher than 95wt%. The growth mechanism of carbon nanofibers and MWNTs was also discussed.     

WS2 超细粉体的固相法合成

WS2 超细粉体的固相法合成;WS2;固相反应;过硫系数;高能球磨;粒度